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IS 13949 (1994): Textile auxiliaries-Dimethylol dihydroxyethylene urea (DMDHEU) reactant [TXD 7: Textile Sizing andFinishing Materials]

TEXTILE AUXILIARIES - DIMETHYLOL DIHYDROXY ETHYLENE UREA (DMDHEU)

REACTANT - SPECIF1CATION

UDC 677-047-6

Q BIS 1991

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHT 110002

March 1994 Price Group 3

Textile Sizing and Finishing Materials Sectional Committee, TX 07

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Textile Sizing and Finishing Materials Sectional Committee had been approved by the Textile Division Council.

Various advantages and disadvantages associated with the use of dimethylol dihydroxy ethylene urea in textile industry are given in Annex A.

For the purpose of deciding whether a particular requirement of this standard is complied with, the fina value, observed or calculated, expressing the result of a test or analysis, shall be rounded off ill accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )‘. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

IS 13949 t 1994

Indian Standard

TEXTILE AUXILIARIES- DIMETHYLOL DIHYDROXYETHYLENEUREA(DMDHBU)

REACTANT-SPECIFICATION 1 SCOPE Table 1 Dimethylol Dihydroxy Ethylene

1.1 This standard specifies the requirements and Urea - Specific Requirements

methods of test for dimethylol dihydroxy ethylene ( Clause 3.2 ) urea ( DMDHEU ) reactant solution used in textile industry. It also specifies details of sl. measurement of crease recovery angle to check N,,.

Characteristic Requirement Method of Test

its effectiveness as cross-linking agent. (1) (2) (3) (4)

2 REFERENCES i) Total solid content 45 % Annex B

2.1 The following Indian Standards are necessary Min ( vi/m )

adjuncts to this standard: ii) PH of solution 7-8 without catalyst IS 1390 : 1983 and 4-5 with

IS No. Title catalyst

188 : 1980 Cotton poplins ( second revision ) iii) Free formaldehyde 1’0 %, Annex C

content, Max

1070 : 1992 Water for general laboratory use iv) Total formaldehyde 33.7 f 2 % Annex D ( third revision ) content

1390 : 1983 Methods for determination of flH “1 Nitrogen content 15.7 f 2 % Annex E

value of aqueous extracts of Annex F textile materials ( jirst revision )

vi) Nitrogen to formal- 1’0 - 1.3 dehyde molar

Method for determination of ratio

4681 : 1981 recovery from creasing of textile vii) Active matter 30% with catalyst

fabrics by measuring the angle of content, Min and 40% without

recovery (first revision ) catalyst

3 REQUIREMENTS 6 MARKING

3.1 General Requirements

The reactant shall be clear transparent solution free from turbidity and shall be of white to pale yellow colour.

6.1 Each package shall be legigly and indelibly marked with the following:

3.2 Specific Requirements

Dimrthylol dihydroxy ethylene urea ( DMDHEU ) shall meet the requirements given in Table 1.

a)

b)

4 CREASE RECOVERY ANGLE

The crease recovery angle of bleached, mercerized white cotton poplin conforming to IS 188 : 1980 treated with the reactant solution by the method prescribed in Annex G shall be 240” Min when tested by the method given in IS 4681 : 1981.

Net mass of the resin solution;

Name of the mater.iaI namely dimethylol dihydroxy ethylene urea

Solid content of the material;

Indication of source of the manufacture; and

Month and year of manufacture.

6.2 BIS Certification Marking

Each package may also be marked with the Standard Mark.

5 PACKING

The material shall be suitably packed in waterproof packages as detailed in the contract or order.

6.2.1 The use of the Standard Mark is governed by the provisions of Bureau of Indian Standards Act, 1986 and the Rules and Regulations made thereunder. The details of conditions under which the licence for the use of Standard Mark

1

18.13949 t i.994

may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards.

7 SAMPLING

7.1 Lot

The quantity of dimethylol dihydroxy ethylene urea solution of one definite composition delivered to a buyer against one despatch note shall constitute a lot.

7.2 Unless otherwise agreed to between the buyer and the seller, the number of packages to be selected from each lot at random shall be as

given below:

Lot Size Sample Size up to 15 3 16 to 25 26 to 50 s 51 to 100 7 101 and above 10

7.3 Draw small quantities of the resin solution by suitable sampling instrument from at least three different parts of each container and mix them thoroughly so as to get a composite sample of desired mass.

7.4 The reactant solution shall be declared, as conforming to the requirements of this standard if all the composite specimen sprepared in 7.3 meet the relevant requirements as specified in 3 and 4.

ANNEX A

( Foreword )

USES, ADVANTAGES AND DISADVANTAGES OF DIMETHYLOL DIHYDROXY ETHYLENE UREA REACTANT

A-l Dimethylol dihydroxy ethylene urea product is not recommended for finishing of white ( DMDHEU ) is extensively used in textile goods. DMDHEU does not affect the light fast- industry for wash and wear and for durable press ness of dyes in general and those of reactive dyes finishing. The finish obtained with DMDHEU in particular. It is an excellent reactant for the exhibits excellent crease recovery and is fast to deferred cure process. It gives low formaldehyde repeated home launderings. However, due to high odour and thus it is convenient to stitch the chlorine damage to finished fabric ( mainly garments from the sensitised cloth. due to impurities present in DMDHEU ), this

ANNEX B

( Clause 3.2.1 and ‘T&e 1 )

METHOD FOR DETERMINATION OF TOTAL SOLID CONTENT OF THE RESIN SOLUTION

B-l APPARATUS

B-l.1 A centrifuge with centrifuge bottles/tubes capable of rotating at 2 500 rev/min.

B-l.2 A Weighing Balance Correct up to 1 mg.

B-2 PROCEDURE

B-2.1 Weigh about 5 g of resin solution exactly in a tared centrifuge bottle/tube. Add to it about 50 ml ( or more depending upon the capacity of the centrifuge bottle ) of acetone and centrifuge at 2 500 rev/min for about 10 minutes when the solid matter separatt s out as a viscous oil.

B-2.2 Decant off the upper layer and add about 50 ml of fresh acetone to the oily residue in the centrifuge bottle and centrifuge at 2 500 rev/min for about 10 minutes. Repeat the process ( 3 to 5 times ) until the resin, free of water, separates out as solid or sticky mass. B-2.3 After removal of acetone, weigh the centrifuge bottle containing the solid resin. B-2.4 Calculate the total percent solid content (S) of the resin by mass of the resin solution by the formula:

S, percent = Mass of solid resin

Mass of resin solution taken x 100

2

IS 13949 : 1994

ANNEX C

( Clause 3.2 and Table 1 )

METHOD FOR DETERMINATION OF FREE FORMALDEHYDE CONTENT OJ? THE RESIN SOLUTION

C-l PRINCIPLE

C-l.1 A sample of the resin solution is reacted with sodium sulphite when free formaldehyde present in the solution forms a formaldehyde bisulphite adduct and sodium hydroxide is libera- ted. The mixture is then titrated with standard hydrochloric acid solution.

H

HCHO + NaZS03 + Hz0 = H-b-OH + NaOH

;

Formaldehyde adduct of NasSOs.

C-2 APPARATUS

a)

b)

A conicaljask - 500-ml capacity.

A weighing balance - with an accuracy up

to 1 mg.

C> A pipette - 25-ml capacity.

d) A burette.

C-3 REAGENTS

C-3.1 Quality of Reagents

Unless specified otherwise pure chemicals shall be employed in tests and distilled water ( see IS 1070 : 1992 ) shall be used where the use of water as reagent is intended.

NOTE - ‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the test results.

a) Sodium Sulphite Solution - 1 M prepared by dissolving 12.6 g of anhydrous sodium sulphite in 100 ml of water.

b) Hydrochloric Acid Solution - 1 N.

c) Thymolphthalein Indicator Solution - Prepared by dissolving 0.1 g indicator in 100 ml of 80 percent rectified spirit.

C-4 PROCEDURE

C-4.1 Take 20 ml of 1 M sodium sulphite solution in a conical flask previously placed in an ice bath. Add to it 3 drops of thymolphthalein indicator.

C-4.2 Neutralize the solution obtained in C-4.1 carefully with 1 N hydrochloric acid until the colour disappears.

C-4.3 Weigh accurately 10 g of resin solution in a beaker and dilute to 100 ml after neutralizing with thymolphthalein.

C-4.4 Add the solution obtained in C-4.3 to the solution obtained in C-4.2.

C-4.5 Titrate the solution obtained in C-4.4 with 1 N hydrochloric acid to complete discoloration.

C-4.6 Calculate the free formaldehyde content (F) percent by mass of the resin solution by the formula:

where

Jv=

v=

F = 3.003 x fl x V

normality of hydrochloric acid used for titration; and

volume in ml of 1 N hydrochloric acid required for titration.

ANNEX D

( Clause 3.2 and Table 1 )

METHOD FOR DETERMINATION OF TOTAL FORMALDEHYDE

CONTENT OF THE RESIN SOLUTION

D-l REAGENTS D-2 PROCEDURE

a) b) 4 4 e)

Sodium Hydroxide Solution -- 2 N.

Iodine Solution - 0.1 N.

Starch Solution

Sulphuric Acid Solution - 2 N.

Sodium Thiosulphate Solution - O-1 N;

D-2.1 Weigh about 0.2 g of resin solution into a 250-ml Eilenmeyer flaik and add to it 10 ml of 2 N sodium hydroxide solution and 50 ml of 0.1 N iodine solution. Let the mixture stand for 1 to 1) hours at 20 f 2°C in the closed flask.

3

IS 13949 I 199il:

D-2.2 Add to this solution 20 ml of 2 N sulphuric where acid and titrate with 0.1 N sodium thiosulphate solution, with stirring to the colourless end point. -v, =

NOTE -The addition of small amount of starch solution makes the end point easier to detect.

D-2.3 Calculate the total formaldehyde content v* = (X) of the resin solution by the formula:

x= 0.15 x ( VI-- Vz) m m=

”

volume in ml of 0.1 N iodine solution taken,

volume in ml of 0. I N sodium thiosulphate required, and

mass of the resin solution taken in g.

ANNEX E

( Clause 3.2 and Tuble 1 )

METHOD FOR DETERMINATION OF NITROGEN CONTENT

E-l APPARATUS

a) A Weighing Bottle

b) Kjeldahl Flask - with a loosely fitting pear shaped hollow glass stopper.

c) A Wuter Bath - capable of working at a temperature of 100 f 2°C.

d) A Volumetric Flask - 100 ml capacity.

e) A Beaker - 250 ml capacity.

f ) Distillation Assembly

E-2 REAGENTS

4 b) c) 4 e) f 1 g) h)

j)

Concentrated sulphuric acid

Sucrose

Selenium catalyst

Potassium sulphate

Copper sulphate

A few pieces of pumice stone

Sulfihuric acid solution - 0.05 N.

Mixed Indicator Solution - obtained by dis- solving 0.2 g methyl red and 0.1 g methylene blue in 100 ml of rectified spirit.

Sodium hydroxide solution - 0.05 N.

E-3 PROCEDURE

E-3.1 Weigh accurately about 0.5 g of the sample in a weighing bottle and transfer it to Kjeldahl flask. Add to it 25 ml of concentrated sulphuric acid and 0.5 g of sucrose.

E-3.2 Keep the Kjeldahl flask in a boiling water bath for one hour and then add 0.1 g selenium, 18 g potassium sulphate and 0.3 g of copper sulphate. Keep the flask in an inclined position and close with a loosely fitting pear shaped hollow glass stopper to prevent loss of’ sulphuric acid or entry of dust. Heat the mixture gently in a fume

cupboard until the initial frothing has ceased. Heat the liquid to boiling point and continue boiling until the solution becomes clear. Boil the liquid for a further period of 2 hours and then cool the contents of the flask.

E-3.3 Transfer the contents of Kjeldahl flask to a loo-ml volumetric flask and make the solution up to the mark. Take 10 ml of this solution in a volumetric flask and add to it a few pieces of pumice stone.

E-3.4 Take 50 ml of sulphuric acid solution ( 0.05 N ) and 3 drops of mixed indicator [ see E-2 (h) ] in a beaker. Set up a distillation assembly. Add excess of sodium hydroxide solution ( 0.05 N ) through the separating funnel and mix the contents of the flask by mild shaking. Distill about one-third of the total volume of the solution in the flask. Wash the dip tube with water, collecting the washing in the beaker.

E-3.5 Titrate the excess of sulphuric acid in the beaker with sodium hydroxide solution ( 0.~5 N ).

E-3.6 Carry out a blank titration without the sample as described from E-3.1 to E-3.4,

E-3.7 Calculate the nitrogen, percent by mass ( JV) by the following formula:

“YE 1.4 ( v,-- VI ) x 0.05 X

100 -. m 10

where

v, =

v, =

volume in ml of sodi.um hydroxide solution ( 0.05 N ) used to mutralize excess of acid in the determination with he sample,

volume of sodium hydroxide solution used in blank titration, and

m = mass in g of the sample taken for test.

4

IS 13949 : 1994

ANNEX I:

( Clause 3.2 and Table 1 )

DETERMINATION OF NITROGEN TO FORMALDEHYDE MOLAR RATIO

F-l Calculate the nitrogen to formaldehyde molar where ratio ( N : F ) of the resin solution by the follow- N = percent nitrogen content of the resin ing formula: solution and 14 represents molecular

weight of nitrogen, and

n/14 Molar ratio = x,3O

X = percent total formaldehyde content of the resin solution and 30 represents molecular weight of formaldehyde.

ANNEX G

( Clause 4 )

METHOD FOR TREATMENT OF COTTON FABRIC WITH DIMETHYLOL DIHYDROXY ETHYLENE UREA

G-l APPLICATION OF RESIN Catalyst ( Magnesium chloride ) = 15 g/l

G-l.1 The resin is applied by pad-dry-cure Wet pick up = 80 y/0 with 2 dips and 2 nips

method and following recipe is used: Fabric is then dried at 80-100°C for 5 minutes Resin = 100 g/l and cured at 150% for 5 minutes.

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Review of Indian Standards

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This Indian Standard has been developed from Dot : No. TXD 7 ( 2323 ).

Ameodments Issued Since Publication

Amend No. Date of Issue Text Affected

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